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The complete report of Analytic Chemistry II experiment with the title

“Extraction Continue of nabati oil.” created by :
Name : Kasturi Indraswari

ID : 1713440004

Group : III

Class : ICP of Chemistry Education

It has been checked and consult by assistant and assistant coordinator this report
has been accepted

Makassar, April 2016

Assistant Coordinator Assistant

Mutmainnah Umar Mutmainnah Umar

Known by

Responsibility Lecturer

Dr. ENG Zulifikar M.T

ID. 19701202 1999802 2 001
A. TITLE OF EXPERIMENT
Extraction Continue of Nabati Oil
B. OBJECTIVES OF EXPERIMENT
1. To extract nabati oil from sample (peanut) by using of soxhlet.
2. To determine oil content from sample by using of distillation.
C. LITERATURE REVIEW
The purpose of an extraction technique is physically to separate
components of a mixture (solutes) by exploiting differences in their relative
solubilities in two immiscible liquids or between their affinities for a solid
sorbent. Substances reach an equilibrium distribution through intimate contact
between the two phases, which are then physically separated to enable the species
in either phase to be recovered for completion of the analysis. An equilibrium
distribution of the solutes between the two phases is established by dissolving the
sample in a suitable solvent, then shaking the solution with a second, immiscible,
solvent or by passing it through a sorbent bed or disk. Where the equilibrium
distributions of two solutes differ, a separation is possible. The principal factors
that determine how a solute will distribute between two phases are its polarity and
the polarities of each phase. Degree of ionization, hydrogen bonding and other
electrostatic interactions also play a part (Kealey, 2002: 109).
A liquid–liquid extraction is one of the most important separation
techniques used in environmental, clinical, and industrial laboratories. Two
examples from environmental analysis serve to illustrate its importance. Public
drinking water supplies are routinely monitored for trihalomethanes (CHCl 3,
CHBrCl2, CHBr2Cl, and CHBr3) because of their known or suspected
carcinogeneity. Before their analysis by gas chromatography, trihalomethanes are
separated from their aqueous matrix by a liquid–liquid extraction using
pentane.21 A liquid–liquid extraction is also used in screening orange juice for the
presence of organophosphorous pesticides. A sample of orange juice is mixed
with acetonitrite and filtered. Any organophosphorous pesticides that might be
present in the filtrate are extracted with petroleumether before a gas
chromatographic analysis. In a simple liquid–liquid extraction the solute is
partitioned between two immiscible phases. In most cases one of the phases is
aqueous, and the other phase is an organic solvent such as diethyl ether or
chloroform. Because the phases are immiscible, they form two layers, with the
denser phase on the bottom. The solute is initially present in one phase, but after
extraction it is present in both phases. The efficiency of a liquid–liquid extraction
is determined by the equilibrium constant for the solute’s partitioning between the
two phases. Extraction efficiency is also influenced by any secondary reactions
involving the solute. Examples of secondary reactions include acid–base and
complexation equilibria (Harvey, 2000: 215).
Distillation is a technique of separating mixture in liquid phase that was
homogenous with way to evaporating process and condenced process and we get
distillate that was more contain volatile component. Boiling liquid is the liquid
that was evaporated by bubbles that was formed in liquid. If adding of heat was
added the velocity of liquid bubbles that was formed also added and evaporation
heat was absorbed (Tim Dosen Kimia Analitik, 2017: 25).
Solvent extraction (SE) is used as a means of sample pre-treatment or
clean-up to separate analytes from matrix components that would interfere with
their detection or quantitation (Topic A4). It is also used to pre-concentrate
analytes present in samples at very low levels and which might otherwise be
difficult or impossible to detect or quantify. Most extractions are carried out
batchwise in a few minutes using separating funnels. However, the efficient
extraction of solutes with very small distribution ratios (<1) can be achieved only
by continuously exposing the sample solution to fresh solvent that is recycled by
refluxing in a specially designed apparatus. Broad classes of organic compounds,
such as acids and bases, can be separated by pH control, and trace metal ions
complexed with organic reagents can be separated or concentrated prior to
spectrometric analysis. Organic compounds with acidic or basic functionalities
dissociate or protonate in aqueous solutions according to the pH of the solution.
Their extraction can, therefore, be in the chemical compound optimized by pH
adjustments (Kealey, 2002: 112).
 The free fatty acid was found to be 5.75 mgKOH/g which is low,
signifying that the oil is edible and can stay for a long time without getting rancid.
The acid value was obtained by multiplying the free fatty acid by 2 giving a value
of 11.50 mgKOH/g. As such cottonseed oil is good for soap production. The
iodine value which gives the degree of unsaturation in vegetable oils was found to
be 94.7g/100g for cottonseed oil. Low moisture content of the oil is advantageous
in terms of storage stability since the lower the moisture content, the better the
storability and suitability to be preserved for a longer period; the oil can be
classified as non-drying based on the value obtained for Iodine value. Also, the
result obtained for the saponification value portends that the oil is good for soap
production. Thus, the oil has great prospects in terms of its edibility, storability
and also suitability for soap production (Adelola, 2012).
D. METHOD OF EXPERIMENT
1. Apparatus
a. Soxhlet 1 unit
b. Condenser liebig 1 unit
c. Round flask 1 unit
d. Condenser Distillation 1 unit
e. Analytical Balance 1 unit
f. Beaker glass 100 ml 1 units
g. Spatula 1 unit
h. Measuring glass 25 ml 1 unit
i. Rough and soft cloth 1 unit
j. Drop pipette 2 units
k. Hotplate 1 unit
l. Stative and clamp 1 unit
m. Spray bottle 1 unit
n. Basin 1 unit
o. Boiling stone 3 unit
p. Hose 2 units
q. Water pump 1 unit
 r. Vapor cup 1 unit
2. Chamicals
a. Pecan
b. Petroleum ether
c. Aquadest (H2O)(aq)
d. Filter paper
e. Strap
f. Ice cubes (H2O)(aq)
g. Aluminum foil (Al2O3)
3. Work Procedures
a. 25 grams of candlenut was crushed with mortar and pestle
b. The refined candlenut was wrapped in filter paper according to the
size of the soaking flask used.
c. The top and bottom of the filter paper were covered with cotton then
put it into a soaking flask and soclet tool.
d. Petrolium ether was put into the godok flask through an immersion
flask as much as 60% of the volume of the pumpkin and add some
boiling stone.
e. The soxhlet tool was assembled
f. Extraction was done by heating pumpkin godok until the solvent
circulation occurs 5 times with a temperature of 50 - 60oC.
g. Distillation was carried out to separate the ether from the residue.
h. The residue was transferred into the evaporating dish and evaporates
until the residue is free of ether odor.
i. The residue was then weighed and the volume is measured to
determine its specific gravity.
j. Oil content was calculated from the sample.
E. EXPERIMENT RESULT
1. Observation result
No. Activity Result
1. Grind candlenut Candlenut texture become
 smooth
Weight 50 grams of smooth
2. 50 grams of candlenut
candlenut
Wrap 50 grams of smooth
3. Smooth candlenut in filter paper
candlenut package into soxhlet
Insert the candlenut package into
4. Candlenut package in soxhlet
soxhlet
Add petroleum ether as much as ¾
5. Petroleum ether in round flask
of the volume of round flask
6. Add boiling stones Boiling stones in round flask
Extraction by heating round flask
7. Circulation accurs 3 time
for 3 hours
8. Distillation until formed the residu Residu like oil and yellow
The residu is evaporated until it is
9. Residu like oil and deep yellow
adorles or free of petroleum ether
10. Measured the volume Volume of oil is 25,7 ml
11. Weight of oil Weight of oil is 20,32 gr
Density of vegetable oil with
12. = 0,8 gr/ml
formula = m/v
2. Data Analysis
Known : Volume of oil = 25,7 mL
Mass of oil = 20,32 gram
Mass of sample = 50 gram
Asked : Density and rendement?
Solution :

20,32 gr
25,7 mL

0,8 gr/mL

Rendement
20,32 gr
50 gr
 X100% = 40%

F. DISCUSSION
Ekstraksi kontinyu minyak nabati ini bertujuan untuk mengekstrak
minyak nabati dari biji kemiri dengan menggunakan soxhlet dan menentukan
kadar minyak dari sampel biji kemiri dengan cara destilasi. Dimana ekstraksi
kontinyu merupakan salah satu metode pemisahan komponen zat dalam
sampel yang memiliki perbedaan distribusi yang relatif kecil, sehingga untuk
pemisahan dilakukan proses ekstraksi berulang-ulang dengan perantaraan
panas oleh setiap tahapan ekstraksi dengan pemanasan (Khopkar, 1990: 107).
Pemanasan pada percobaan ini merupakan perantaraan untuk menguapkan zat
pelarut.
Percobaan dimulai dengan menggerus biji kemiri yang berfungsi
untuk memudahkan pelarut dalam mengikat ekstrak minyak nabati yang
terkandung dalam sampel karena seluruh bagian sampel terendam oleh
pelarut dengan kata lain luas permukaan yang semakin besar menyebabkan
tumbukan yang terjadi semakin banyak sehingga sampel kemiri terekstrak
secara maksimal. Kemudian ditimbang dan dibungkus dengan kertas saring
biasa agar pada saat sokletasi sampel kemiri tidak terhambur, dan juga kertas
saring biasa dipilih karena memiliki pori-pori yang besar sehingga kemiri
dapat terekstraksi dengna baik. Kemudian kemiri yang dibungkus diikat agar
kertas saring yang dijadikan pembungkus tidak terlepas.
Kamiri yang telah dibungkus kemudian dimasukkan ke dalam soxhlet.
Kemudian memasukkan batu mendidih ke dalam labu bundar, batu didih
berfungsi untuk meratakan panas dan mengurangi ledakan karena batu didih
memiliki pori-pori yang dapat menyerap panas. Kemudian ditambahkan eter
melalui bagian atas soxhlet. Eter dipilih sebagai pelarut karena menurut
Anwar dkk (2016, 85) eter adalah pelarut yang relative non-polar, dimana
minyak nabati juga memiliki sifat non-polar sehingga merupakan pelarut
yang baik untuk minyak nabati karena memiliki kepolaran yang sama. Selain
itu, eter juga memiliki titik didih rendah yaitu 40-60°C (MSDS, 2017: 1)
sehingga dapat dengan mudah menguap dan mempercepat ekstraksi.
Kemudian dilakukan pemanasan dan ekstraksi. Dalam praktikum ini
ekstraksi kontinyu yang dilakukan adalah sokletasi. Menurut Leba (2017: 4-
5) sokletasi adalah salah satu jenis ekstraksi menggunakan soxhlet. Ekstraksi
dilakukan dengan memanaskan pelarut dalam hal ini ialah eter, uap pelarut
yang dihasilkan terhubung dengan pendinginan dalam kondensor dan terus
menerus akan membasahi sampel dan secara teratur pelarut dimasukkan
kembali ke dalam labu dengan membawa analit, proses ini berlangsung terus
menerus.
Prinsip dasar dari percobaan ini adalah ekstraksi kontinyu
menggunakan perantara panas, sedangkan prinsip kerjanya adalah pemisahan
zat dalam sampel menggunakan pelarut berulang. Sirkulasi dilakukan tiga
kali yang berfungsi agar ektraksi minyak nabati dari kemiri ini menghasilkan
hasil yang banyak.
Setelah melakukan ektraksi dengn soxhlet, larutan pada labu bundar
kemudian dipindahkan ke labu destilasi untuk melakukan destilasi. Distilasi
adalah istilah sederhana, penguapan diikuti oleh kondensasi. Ini adalah
metode pemisahan komponen solusi yang relatif mudah
menguap (Thakore and Bharat, 2007: 378). Tujuan dari destilasi ini ialah
untuk memisahkan minyak nabati dari hasil ektraksi tersebut dengan
pelarutnya yaitu eter berdasarkan perbedaan titik didihnya. Prinsip dasar
destilasi ialah pemisahan dua zat cari berdasarkan titik didihnya, adapun
prinsip kerja destilasi adalah pemanasan, penguapan dan pengembunan dari
suatu zat cair pada tekanan dan suhu tertentu. Proses destilasi dilakukan
sampai potreleum eter telah terpisah secara sempurna yang ditandai dengan
destilat berwarna bening dan ekstrak minyak nabati pada labu destilasi
berwarna kuning. Pada destilasi ini larutan yang terlebih dahulu keluar ialah
eter karena memiliki titik didih yang lebih rendah.
Setelah warna residu pada abu destilasi berubah warna menjadi
kuning, kemudian dilakukan lagi penguapan, penguapan dilakukan agar eter
 benar-benar menguap dan tidak terkandung dalam minyak nabati lagi dan
minyak nabati yang didapat murni. Penguapan dilakukan hingga bau eter
tidak tercium lagi. Setelah dilakukan pengupan maka minyak nabati dari
kemiri telah didapatkan, kemudian minyak nabati tersebut dihitung berapa
volumenya dan dilakukan perhitungan rendamen. Dari hasil percobaan,
diperoleh residu berwarna kuning dengan berat 20,32 gram dengan volume
25,7 mL. Kemudian dari hasil analisis data massa jenis minyak nabati sebesar
0,8 g/mL selain itu diperoleh kadar minyak dalam sampel sebesar 40%.
Rendamaen yang dihasilkan kurang dan hal tidak sesuai dengan teori dimana
menurut (Suwarto dkk, 2014: 78) minyak rendemen yang diperoleh biasanya
30-65% .
G. CONCLUSION
Based on this experiment, we can conclude that:
1. Vegetable oil can be obtained by extraction using Soxhlet and
distillation apparatus with ether solvents
2. The oil content in the sample was 40%
 BIBLIOGRAPHY

Adelola, O.B, and Efomah, A.N. 2014. Extraction and Characterizatio of

Cottonseed (Gossypium) Oil. Journal of basic and applied science. Vol 1.
No 2

Harvey, David. 2000. Modern Analytical Chemistry. America: McGraw-Hill.

Kealey, D and Haines, P.J. 2002. Analytical Chemistry. London. BIOS.

Tim Dosen Kimia Analitik. 2015. Penuntun Praktikum Kimia Analitik II.
Makassar: FMIPA Universitas Negeri Makassar